CN108218467B - Preparation method of porous nano silicon carbide ceramic with high porosity and low thermal conductivity - Google Patents
Preparation method of porous nano silicon carbide ceramic with high porosity and low thermal conductivity Download PDFInfo
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 55
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000005543 nano-size silicon particle Substances 0.000 title claims abstract description 15
- 239000000919 ceramic Substances 0.000 title claims description 22
- 238000002360 preparation method Methods 0.000 title claims description 12
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000011148 porous material Substances 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002002 slurry Substances 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 239000002105 nanoparticle Substances 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- 239000010439 graphite Substances 0.000 claims abstract description 8
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000003825 pressing Methods 0.000 claims abstract description 4
- 238000012216 screening Methods 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 11
- 238000005245 sintering Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 3
- 238000001272 pressureless sintering Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 description 6
- 238000009413 insulation Methods 0.000 description 4
- 239000011858 nanopowder Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229910018540 Si C Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000004964 aerogel Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005262 decarbonization Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
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- C04B38/063—Preparing or treating the raw materials individually or as batches
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
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Abstract
The invention relates to the field of porous ceramic materials, in particular to a method for preparing a porous nano silicon carbide ceramic material with high porosity and low thermal conductivity by a pore-forming agent method, which comprises the steps of taking β -SiC nano particles and micron flake graphite as raw materials, taking ethanol as a medium, carrying out ball milling and mixing to form slurry, drying the slurry, screening the slurry into powder, pressing the powder into a blank by a mould, further densifying the blank under cold isostatic pressure, carrying out high-temperature pressureless sintering on the blank in an argon atmosphere, and then carrying out heat treatment in the air to remove the pore-forming agent graphite to obtain the porous nano silicon carbide ceramic material with micron pores and nano pores‑1K‑1) The porous nano SiC ceramic material.
Description
Technical Field
The invention relates to the field of porous ceramic materials, in particular to a method for preparing a porous nano silicon carbide ceramic material with high porosity and low thermal conductivity by a pore-forming agent method.
Background
Leading-edge technology applications in thermal insulation and energy conversion at high temperatures require new materials with low thermal conductivity and high reliability. Nanostructured materials have become a research hotspot in the academic and technical fields due to their good thermal insulation properties. The basic mechanism of their thermal resistance arises from the enormous interfacial thermal resistance in nanostructures. However, as the particle size decreases, the specific surface area of the material increases, resulting in a dramatic decrease in the high temperature thermal stability of the nanostructure. The oxide nano-materials mainly applied at present are as follows: silicon dioxide (SiO)2) And alumina (Al)2O3) Aerogel and its composite material, its thermal stability is less than 1200 ℃. Therefore, the bottleneck problem to be solved at present is how to achieve both extremely low thermal conductivity and high thermal stability in the novel nanomaterial.
The silicon carbide ceramic can show excellent mechanical property and corrosion resistance in a severe high-temperature environment, so that the silicon carbide ceramic has wide application in the industrial field. More importantly, due to the strong Si-C covalent bond and low self-diffusion coefficient, it was reported that cold pressed prepared SiC powder bulk can maintain its room temperature initial sample size at high temperature of 1800 ℃ without severe shrinkage (m.fukushima et al. mater.sci.eng.b 2008(148): 211-. And beta-SiC has ultrahigh phase stability and no phase transition within 2000 ℃ (B.K.Jang et al.adv.Mater.2007(8):655 and 659). While SiC is a high thermal conductivity ceramic, nano SiC exhibits surprising thermal insulation properties when the particle size is reduced to the nanometer scale (p.wan et al.script mater.2017(128): 1-5). Therefore, the porous nano silicon carbide ceramic is a high-temperature-resistant thermal insulation and thermal protection material with great potential and applied to the fields of aviation and aerospace.
Disclosure of Invention
The invention aims to provide a preparation method of porous nano silicon carbide ceramic with high porosity and low thermal conductivity, so that the SiC porous ceramic has the brand-new characteristic of low thermal conductivity.
The technical scheme of the invention is as follows:
a preparation method of porous nanometer silicon carbide ceramic with high porosity and low thermal conductivity is provided, wherein the silicon carbide material is porous nanometer SiC ceramic, and the preparation method comprises the following specific steps:
1) preparing slurry: preparing raw materials by using beta-SiC nano particles and graphite powder in a mass ratio of 9: 1-5: 5, and performing ball milling and mixing for 8-16 hours by using ethanol as a medium to form slurry;
2) drying the slurry, screening into powder, pressing into a blank by using a die, and further densifying under the cold isostatic pressure of 200-240 MPa for 10-30 minutes;
3) and (3) sintering the blank body at high temperature and no pressure for 1-3 hours in an argon atmosphere at 1400-1600 ℃, and then carrying out heat treatment for 3-5 hours at 600-800 ℃ in the air to remove the pore-forming agent graphite, so as to obtain the porous nano silicon carbide ceramic material with micropores and nanopores.
According to the preparation method of the porous nano silicon carbide ceramic with high porosity and low thermal conductivity, the porosity range of the porous nano SiC ceramic material is 54-76%, the micropores are uniformly distributed in a flake shape, and the pore size is as follows: 2 μm to 6.5 μm, thickness: 0.5 to 1.5 μm; the nano-pores are distributed on the framework of the ceramic material, and the pore diameter range is less than 50 nm.
In the preparation method of the porous nano silicon carbide ceramic with high porosity and low thermal conductivity, β -SiC nano particles have the average particle size of20-50 nm, and the particle size distribution of the graphite powder is D90＝6.5μm。
The preparation method of the porous nano silicon carbide ceramic with high porosity and low thermal conductivity has the following temperature rise rate in high-temperature sintering: 8 to 12 ℃/min at a temperature below 1000 ℃ and 4 to 6 ℃/min at a temperature above 1000 ℃.
The invention has the advantages and beneficial effects that:
1. the invention provides a method for preparing a porous nano silicon carbide ceramic material with high porosity and low thermal conductivity by a pore-forming agent method, and the method can be used for preparing SiC porous ceramic with both micropores and nanopores and controllable porosity, high porosity and low thermal conductivity.
2. The invention has convenient operation and only needs to carry out the processes of slurry preparation, compression molding, high-temperature sintering, decarbonization treatment and the like.
3. The invention does not need special equipment and is easy for large-scale production.
4. The porous nano SiC ceramic material with higher porosity can be prepared by the method, has a multi-level nano structure heat-resistant mechanism and a multi-level pore structure, can greatly reduce the thermal conductivity, and is a light high-temperature-resistant heat-insulating material with excellent performance.
In a word, β -SiC nano particles and micron flake graphite are used as raw materials, after 12-hour ball milling, uniformly mixed powder is obtained, after 220MPa cold isostatic pressing forming, pressureless sintering is carried out for 2 hours in 1500 ℃ argon atmosphere, then a sample is subjected to heat treatment for 4 hours at 700 ℃ in the air, a graphite pore-forming agent is removed, and finally the porous nano SiC ceramic is prepared-1K-1) The porous nano SiC ceramic material.
Drawings
FIG. 1 is a transmission electron micrograph of the SiC nanopowder of example 1. In the figure, the upper inset is a morphology of a single SiC nanoparticle at high magnification; the lower inset is the overall morphology of the SiC nanopowder at low magnification.
Fig. 2(a) is an X-ray diffraction three-dimensional imaging (XRT) diagram of the porous nano-SiC ceramic material in example 2.
Fig. 2(b) is a Scanning Electron Microscope (SEM) photograph of the porous nano-SiC ceramic material in example 2.
Detailed Description
In the specific implementation process, the preparation method of the porous nano silicon carbide (SiC) ceramic with high porosity and low thermal conductivity comprises the following specific steps:
1) preparing raw materials of β -SiC nano particles and graphite powder in mass ratios of 9:1, 8:2, 7:3, 6:4 and 5:5 respectively, and performing ball milling and mixing for 12 hours by taking ethanol as a medium to form slurry, wherein the average particle size of β -SiC original powder is 35nm, and the particle size distribution of the graphite powder is D90＝6.5μm。
2) Drying the slurry, screening into powder, pressing into a blank by using a mould with a required shape, and further densifying under the cold isostatic pressure of 220 MPa;
3) and (3) sintering the blank at 1500 ℃ in an argon atmosphere at high temperature and without pressure, and then removing the pore-forming agent graphite by heat treatment at 700 ℃ in the air to obtain the SiC porous ceramic material with both micropores and nanopores. The porosity range of the porous nano SiC ceramic material is 54-76%, the micropores are in a flake shape and are uniformly distributed, and the pore size is as follows: 2 μm to 6.5 μm, thickness: about 0.7 μm, nano-pores on the skeleton, and pore diameter less than 50 nm.
The present invention is described in detail below by way of examples.
Example 1
Placing a small amount of SiC nano powder into ethanol, performing ultrasonic dispersion for 30 minutes, then sucking a mixed solution of the powder and the ethanol by using a glass capillary, then dripping 2-3 drops of the mixed solution onto a 200-mesh micro-grid supporting film, fully drying, and observing under a transmission electron microscope, as shown in figure 1. The results in this example show that the average particle size of the β -SiC nanoparticles is about 35nm and the particles contain a large number of stacking faults. The fine particle size produces large interface and grain boundary thermal resistance, and lattice defects (such as stacking faults) further hinder the transmission of heat phonons, thereby effectively reducing the thermal conductivity.
Example 2
Preparing raw materials of beta-SiC nano particles and graphite powder according to the mass ratio of 7:3, and performing ball milling and mixing for 12 hours in a silicon nitride ball milling tank by taking ethanol as a medium to form slurry; then, the slurry is dried and sieved into powder, the powder is pressed into a blank by a mould with a required shape, and the blank is further densified under the cold isostatic pressure of 220MPa for 10 minutes;
and (3) sintering the blank at 1500 ℃ in an argon atmosphere at high temperature and without pressure for 2 hours, and then carrying out heat treatment in the air at 700 ℃ for 4 hours to remove the pore-forming agent graphite, thus obtaining the porous nano SiC ceramic material. In this example, the sample had a porosity of 66.8% and a thermal conductivity of 0.42W m-1K-1. The microstructure of the porous ceramic is shown by the XRT photograph in FIG. 2(a), and the micropores are uniformly distributed in a flake shape and have the pore size of length and width: 2 μm to 6.5 μm, thickness: 0.7 μm. The SEM photograph of FIG. 2(b) shows that nanopores exist between particles in a pore size range of less than 50 nm.
The embodiment result shows that the method combines the nano powder with the pore-forming agent method with simple process, the porosity can be controlled by adjusting the addition amount of the pore-forming agent, the porous nano SiC ceramic prepared by the method has higher porosity and low thermal conductivity, and the porous ceramic with micron pores and nano pores can be prepared.
Claims (2)
1. A preparation method of porous nanometer silicon carbide ceramic with high porosity and low thermal conductivity is characterized in that a silicon carbide material is porous nanometer SiC ceramic, and the preparation method comprises the following specific steps:
1) preparing slurry: preparing raw materials by using beta-SiC nano particles and graphite powder in a mass ratio of 9: 1-5: 5, and performing ball milling and mixing for 8-16 hours by using ethanol as a medium to form slurry;
2) drying the slurry, screening into powder, pressing into a blank by using a die, and further densifying under the cold isostatic pressure of 200-240 MPa for 10-30 minutes;
3) sintering the blank body at the high temperature and no pressure for 1-3 hours in the argon atmosphere at 1400-1600 ℃, and then carrying out heat treatment at the temperature of 600-800 ℃ for 3-5 hours in the air to remove the pore-forming agent graphite, so as to obtain the porous nano silicon carbide ceramic material with micropores and nanopores;
the porosity range of the porous nano SiC ceramic material is 54-76%, the micropores are in a flake shape and are uniformly distributed, and the pore size is as follows: 2 μm to 6.5 μm, thickness: 0.5 to 1.5 μm; the nano-pores are distributed on the framework of the ceramic material, and the pore diameter range is less than 50 nm;
β -SiC nano particles have an average particle size of 20-50 nm and graphite powder has a particle size distribution of D90=6.5 μm。
2. The method for preparing the high porosity and low thermal conductivity porous nano silicon carbide ceramic according to claim 1, wherein the temperature rise rate of the high temperature sintering is as follows: 8 to 12 ℃/min at a temperature below 1000 ℃ and 4 to 6 ℃/min at a temperature above 1000 ℃.
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| CN111947345A (en) * | 2020-07-17 | 2020-11-17 | 浙江吉成新材股份有限公司 | Water refrigeration method and water refrigeration device using porous material |
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| CN103086732A (en) * | 2013-01-21 | 2013-05-08 | 天津师范大学 | Fiber enhanced silicon carbide porous ceramic and preparation method and application thereof |
| CN104496480A (en) * | 2014-12-08 | 2015-04-08 | 中国建筑材料科学研究总院 | Silicon carbide ceramic preform, aluminum-based silicon carbide ceramic material, and preparation method of silicon carbide ceramic preform |
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